Comfort melamine fabrics and process for making them

ABSTRACT

Fabrics made of melamine fibers are made more comfortable by submerging them for at least 20 minutes in a dyebath or mock dyebath that is at least 70° C.

FIELD OF THE INVENTION

The present invention relates to fabrics and yarns made from melaminefibers and processes for imparting physical characteristics, such ascolor, moisture regain and improved hand to them.

BACKGROUND OF THE INVENTION

Melamine fibers are useful in applications requiring resistance to heatand flame. Examples of such applications include upholstery, draperymaterial, fire fighting apparel, etc. Such applications might beconsidered so utilitarian because of their role in preserving life andproperty that appearance is a minor secondary consideration. This is nottrue, however, and style plays an important part of fabric selection.Therefore, it is important that the fabrics made with melamine bedyeable to desired shades. Because the chemistry of the melamine fiberis different than the more commonplace man-made synthetic fibers, thedyestuffs known to dye these more common fibers do not necessarily dyemelamine fibers. As a result, there is a need to find dyestuffs andconditions that will dye the melamine fabrics.

Many melamine fabrics in their natural state may have a harsh or itchyhand. In certain applications of melamine fabrics, this characteristicis viewed as a drawback to using melamine fabrics even when theprotective performance is superior. Methods to increase the comfort andimprove the hand of melamine fabrics are desirable.

Comfort may also be linked to "moisture regain" so that for somefabrics, one method for improving comfort is to increase "moistureregain". It is believed that the ability of a synthetic fiber to absorbmoisture makes such fibers more like cotton and less synthetic feelingagainst the skin. Moisture regain refers to the characteristic offabrics to absorb moisture. Cotton fabrics, which are traditionallyviewed as comfort fabrics, have relatively high moisture regainproperties (typically in the range of about 8.5 to about 10.5) whichallows wicking action to remove moisture from the skin resulting in acomfortable "feel".

Softness is an attribute of hand that some consider to defyquantitation. However, when manually comparing the softness of twodifferent fabrics, there is general agreement on which one is softer.

Melamine fibers are often blended with other fibers such that mostmelamine fabrics are actually blends of melamine and other types offiber. Melamine fibers are blended with a large variety of fibers, forexample, p-aramids, m-aramids, glass, flame resistant (FR) cellulosicfibers, steel, cotton, wool, polyester, etc. The same concerns ofdyeability and hand apply to fabrics made from blends of melamine fibersand other fibers as apply to all melamine fabrics. Methods for dyeingthese fabrics and also improving the hand are desirable.

In addition, novel color effects are sought in the industry. Dyeingmethods that cause unique or attractive appearances in the fabricsubjected to the method are considered beneficial. One popular coloreffect is called "chambray". Chambray fabrics are exemplified by worndenim jeans. Usually, this effect is accomplished by process steps,e.g., stone washing, after the dyeing process. In addition, the denimeffect is usually achievable with dyes that do not exhibit goodwashfastness to cellulosic materials combined with the use of undyedwarp yarns in the starting fabric. Upon washing, certain dyes exhibitpoor fastness to washing resulting in a lighter appearance and morenoticeable uncolored warp yarns.

SUMMARY OF THE INVENTION

It is an object of the present invention to provide a method for dyeingmelamine fabrics.

It is another object of the present invention to provide a dyed melaminefiber fabric.

It is a further object of the present invention to provide a method fordyeing melamine fiber blend fabrics.

It is a still further object of the present invention to provide a dyedmelamine fiber blend fabric.

It is yet another object of the present invention to provide a method toimprove the hand of melamine fiber and melamine fiber blend fabrics.

It is still another object of the present invention to provide amelamine or melamine blend fabric with good hand characteristics.

These and related objects and advantages are achieved with a process forimproving the comfort of fabrics made from melamine fibers by submergingthe fabrics in an aqueous bath heated to more than 70° C. for more than20 minutes. The aqueous bath may be substantially all water or it may bea dyebath. The aqueous bath may contain one or more solutes selectedfrom leveling agents; dispersing agents; chelating agents; lubricatingagents; pH adjustment agents; and combinations thereof. The bath ispreferably heated to a temperature from about 90° C. to about 130° C.The fabric may comprise a blend of melamine fibers and other fibers. Themelamine fibers are preferably melamine-formaldehyde fibers comprisingthe condensation product of melamine and formaldehyde in a molar ratioof two moles of formaldehyde to one mole melamine and containinghydroxyoxaalkylmelamines and, optionally, other additives in smallamounts.

The present invention also includes a process for improving the comfortof fabrics made from melamine fibers by submerging the fabrics in anaqueous bath at a temperature and for a time such that the moistureregain of the melamine fiber in the fabric after said submerging isgreater than about 6.5% by weight and preferably greater than about 7%by weight.

Another aspect of the present invention is a fabric comprising melaminefibers having a moisture regain of greater than about 6.5% by weight andpreferably greater than at least about 7% by weight of the melaminefiber in the fabric. The fabric may be dyed. It may be composed ofmelamine fibers and other fibers.

Related objects and advantages of the present invention will be apparentto those of ordinary skill in the art after reading the followingdetailed description.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

To promote an understanding of the principles of the present invention,descriptions of specific embodiments of the invention follow andspecific language is used to describe the same. It will be understoodthat no limitation of the scope of the invention is intended by the useof this specific language and that alterations, modifications,equivalents and further applications of the principles of the inventiondiscussed are contemplated as would normally occur to one ordinarilyskilled in the art to which the invention pertains.

The following detailed description of the present invention refers todyeing articles in the form of fabrics, yarns, etc. It is believed thatthere is no limitation of the particular form the article may take,i.e., it may be in fabric, yarn, web, thread, fiber, sliver, tow, etc.,form. The invention relates to standard methods for imparting color tofiber in all of these constructions, e.g., dyeing, printing, etc.Preferably, the process is a dyeing process. The dyeing process may bein an aqueous or non-aqueous bath. Currently, an aqueous bath ispreferred.

The melamine fiber may be used alone or it may be blended with anotherfiber to make a mixed component yarn. All-melamine fiber yarns may bemade into fabrics without other types of fibers or with other types offibers, etc. The terms "fabric" and "yarn" and "fiber" should beconsidered interchangeable and given their broadest interpretationconsistent with the art for the purposes of the present invention.

For the purposes of describing the dyeing effects achieved with thepresent invention, the terms "dyed" (and related words) and "stained"(and related words) are used to describe different responses to aparticular dyestuff. These terms are used in accordance with the generalmeaning given to them by those who are ordinarily skilled in this art.

The present invention concerns dyed heat and flame resistant fabrics. Ingeneral, such fabrics as used in this context are those having alimiting oxygen index of greater than about 28 as measured byASTMD-2863-77, more preferably at least 30.

I. DYED FABRICS (AND YARNS) FROM MELAMINE FIBERS AND BLENDS THEREOF(MELAMINE DYED)

One aspect of the present invention is a process for dyeing an articleconstructed from at least a fraction of heat and flame resistantmelamine fiber. The article to be dyed is placed for about 30 to about120 minutes in a dyebath containing a dye or blend of dyes that isheated to at least about 95° C. to about 150° C. This aspect of thepresent invention and articles made thereby are illustrated in Examples1-6.

The article may be composed of 100% melamine fiber or it may be a blendof melamine with other fibers selected from: m-aramid fibers, p-aramidfibers, glass fibers, carbon fibers, other mineral or ceramic fibers,steel fibers, polybenzimidazole fibers, polyimide fibers,polyamide-imide fibers, polytetraflouroethylene fibers,polyetheretherketone fibers, polyacrylate fibers, polyaryletherketonefibers, novoloid fibers, polyethersulfone fibers, poly(vinyl chloride),poly(vinylidene chloride) fibers, liquid crystalline polyester fibers,and blends and combinations of these.

Further, the process of the present invention can be used to dyemelamine fibers that are blended with other fibers that are precolored.Example 2 below demonstrates the process of the present inventionresulting in an even coloring of fabric that is a 60:40 blend ofp-aramid fibers and melamine fibers where the p-aramid fibers werepigmented (sometimes called "producer-colored") black.

The fabric may be in any form: woven, nonwoven, knitted, etc. If thefabric is a blend of melamine with other fibers, the blend level may befrom about 20% to nearly 100% melamine fiber by weight. Preferably, theamount of melamine fiber in the blend will be no more than about 60% byweight.

The melamine fiber may be any melamine fiber, but is preferably amelamine-formaldehyde fiber that is essentially the condensation productof melamine and formaldehyde in a molar ratio of two moles offormaldehyde to one mole of melamine and containinghydroxyoxaalkylmelamines and, possibly, other additives in smallamounts. One suitable melamine fiber is Basofil® fiber available fromBASF Corporation, Mt. Olive, N.J.

The dyestuff in the dye bath is one or more of the following types ofdyes: direct dyes, non-metallized acid dyes, metallized acid dyes,disperse dyes (without carriers) and blends thereof. Other materials maybe present in the dyebath according to conventional dyeing practice.These materials include, for example, leveling agents, anti-foamingagents, dispersing agents, lubricating agents and chelating agents andcombinations of these.

The temperature of the dyebath is in the range of about 95° C. to about150° C., preferably about 110C. to about 150° C. in the case of dispersedyes. The precise temperature will depend on the dyestuff used andshould be readily determinable by those of ordinary skill in the art.

The fabric will be exposed to the dyebath for a period of time that willalso depend on the dyestuff and will be readily determinable by those ofordinary skill in the art. Typical times range from about 30 to about120 minutes.

After the dyeing step is complete and the fabric or yarn is dyed to thedesired shade, typical, optional, subsequent steps may be used. Forexample, after scouring may be used if desired for a particular result.

Surprisingly, it was discovered that when the fabric is a blend ofmelamine fibers with one of the other types of fibers listed above, aunique chambray appearance resulted in the dyed fabric without anysubsequent process steps (e.g., stone-washing) that are often used toenhance a chambray effect. Surprisingly, the melamine fiber is dyed butthe other fiber is not dyed to a significant degree (although, in somecases, it may stain slightly). The fabric, therefore, exhibits achambray appearance without further process steps. It was especiallynotable when other non-melamine heat and flame resistant fibers that arenon-dyeable, i.e., that do not dye to a deep shade (if at all) under thedyebath conditions that are present.

Another related aspect of the present invention is a dyed melamine ormelamine blend fabric. This fabric may be made according to the aboveprocess and will preferably be made from a blend of melamine fibers withother fibers.

The present invention includes a process for dyeing an articleconstructed from heat and flame resistant melamine fiber and proteinfibers. The melamine and protein article to be dyed is placed for about30 to about 120 minutes in a dyebath containing a disperse dye or dyesthat is heated to at least about 95° C. to about 110° C.

The article is a blend of melamine fibers with protein (or animal)fibers selected from: wool, silk, cashmere, mohair, rabbit, etc.) andblends and combinations of these with each other or with other types offibers. The blend may contain from about 20% to nearly 100% melaminefibers by weight.

As noted, the dye preferably used is one ore more disperse dyes andblends thereof. Other materials may be present in the dyebath accordingto conventional dyeing practice. These materials include, for example,leveling agents, anti-foaming agents, dispersing agents, lubricatingagents and chelating agents and combinations of these.

The temperature of the dyebath is preferably in the range of about 95°C. to about 110° C. The precise temperature will depend on the dyestuffused and should be readily determinable by those of ordinary skill inthe art.

The fabric will be exposed to the dyebath for a period of time that willalso depend on the dyestuff and will be readily determinable by those ofordinary skill in the art. Typical times range from about 30 to about120 minutes.

After the dyeing step is complete and the fabric or yarn is dyed to thedesired shade, typical, optional, subsequent steps may be used. Forexample, after scouring may be used if desired for a particular result.

Surprisingly, the blend of melamine fibers with one or more proteinfibers exhibits a unique chambray appearance when dyed with dispersedyes (no carrier). No subsequent process steps were required. By way ofillustration, Examples 6A-6B below describe the dyeing of amelamine/wool blend fabric with a disperse dye wherein the wool does notdye to any significant degree (although it may stain slightly), and thefabric exhibits a pleasing chambray appearance.

Another related aspect of the present invention is a dyed melaminefiber/protein fiber blend fabric. This fabric may be made according tothe above process for dyeing melamine fiber/protein fiber blends andexhibits a chambray appearance.

II. DYED FABRICS (AND YARNS) FROM BLENDS OF MELAMINE FIBERS ANDCELLULOSIC FIBERS (CELLULOSE DYED)

Another aspect of the present invention is a process for dyeing articlesthat are composed of melamine fibers and cellulosic fibers. This processprovides such articles to an aqueous dyebath where it is dyed at atemperature of less than about 95° C. It is not necessary to weave thefabric using one fiber type as a warp and the other as the weft (as withdenim fabrics) to obtain this result. This aspect of the invention andthe fabrics made thereby are illustrated in Examples 7A-7F.

Exemplary cellulosic fibers are natural and synthetic cellulosic fiberssuch as cotton fibers, rayon fibers, bast fibers, leaf fibers, celluloseacetate fibers and blends thereof. These fibers may or may not be flameretardant ("FR") from treatments thereto that are known for the fibertype.

The melamine fiber may be any melamine fiber but is preferably amelamine formaldehyde fiber that is essentially the condensation productof melamine and formaldehyde in a molar ratio of two moles offormaldehyde to one mole of melamine and containinghydroxyoxaalkylmelamines and other additives in small amounts. Onesuitable melamine fiber is Basofil® fiber available from BASFCorporation, Mt. Olive, N.J.

The dyestuff is selected from the group of direct dyes, azoic dyes,reactive dyes, vat dyes, sulfur dyes, napthol dyes, disperse dyes in thecase of acetates, and blends thereof. The preferable dyestuff willdepend on the particular type (or types) of cellulosic fiber used. Othermaterials may be present in the dyebath according to conventionalpractice. For example, to dye cotton fibers with direct dyes, salt (suchas Glauber's Salt) is usually required.

The fabric may be in any form, woven, nonwoven or knitted. It maycontain between about 20% and nearly 100%, preferably, between about 20%and about 80%, melamine fiber by weight. Where the cellulosic fiber isFR cotton, the preferred amount of melamine in the fabric or yarn isabout 20% to about 50% by weight. Other types of fibers may also bepresent.

Pre-dyeing steps, such as scouring, bleaching, mercerizing, etc., may beused as desired. For dyeing, the temperature of the dyebath will be lessthan about 95° C., but the precise temperature will depend on theparticular dyestuff used and will be readily determinable by those ofordinary skill in the art.

The fabric should be exposed to the dye long enough for the fabric todye to the desired shade. The amount of time will depend on the exactcomposition of the fabric and will be readily determinable by thoseordinarily skilled in the art.

Following dyeing, typical aftertreatments may be used as are presentlyknown to those of ordinary skill in the art or are hereafter developed.These steps depend on the specific dyestuff or blend of dyestuffs usedand include, for example, after-scouring, oxidation and neutralization.

Another aspect of the present invention is a heat and flame resistantchambray fabric that contains from about 20% to nearly 100% melaminefibers by weight that are substantially undyed (although they could beprecolored during the fiber making process). In addition to the melaminefiber, the fabric contains cellulosic fibers selected from cottonfibers, rayon fibers, bast fibers, leaf fibers, cellulose acetate fibersand blends thereof with each other or other fibers. The cellulosicfibers are dyed with dyes selected from direct dyes, non-metallized aciddyes, reactive dyes, napthol dyes, vat dyes, sulfur dyes, azoic dyes,disperse dyes (for acetates), and blends thereof.

III. DYED FABRICS (AND YARNS) FROM BLENDS OF MELAMINE FIBER ANDCELLULOSIC FIBER (MELAMINE DYED)

Another aspect of the present invention is a process for dyeing articlesthat are composed of melamine fibers and cellulosic fibers wherein themelamine fiber is dyed. This process provides such fabrics to an aqueousdyebath where it is dyed at a temperature exceeding about 95° C.Surprisingly, the melamine fiber is dyed but the cellulosic fiber is notsubstantially dyed (it may be stained) so that the fabric exhibits achambray appearance without further process steps. It is not necessaryto weave the fabric using one fiber type as a warp and the other as theweft (as with denim fabrics) to obtain this result. This aspect of theinvention and the fabrics made thereby are illustrated in Examples8A-8D.

Exemplary cellulosic fibers are natural and synthetic cellulosic fiberssuch as cotton fibers, rayon fibers, bast fibers, leaf fibers, andblends thereof with each other and with other fibers. These fibers mayor may not be flame retardant (FR) from treatments thereto that areknown for the fiber type.

The melamine fiber may be any melamine fiber but is preferably amelamine formaldehyde fiber that is essentially the condensation productof melamine and formaldehyde in a molar ratio of two moles offormaldehyde to one mole of melamine and containinghydroxyoxaalkylmelamines and, possibly, other additives in smallamounts. One suitable melamine fiber is Basofil® fiber available fromBASF Corporation, Mt. Olive, N.J.

The dyestuff is selected from the group of direct dyes (without salt,e.g., Glauber's Salt), metallized acid dyes, non-metallized acid dyes,disperse dyes, and blends thereof. Other materials may be present in thedyebath according to conventional practice.

A fabric may be in any form, woven, nonwoven or knitted. It may containbetween about 20% and nearly 100% by weight, preferably, between about20% and about 80%, melamine fiber by weight. Where the cellulosic fiberis FR cotton, the preferred amount of melamine in the fabric or yarn isabout 20% to about 50% by weight.

Predyeing steps, such as scouring, bleaching, mercerizing, etc., may beused as desired. For dyeing, the temperature of the dyebath will be fromat least about 95° C. to about 150° C., but the precise temperature willdepend on the particular dyestuff used and will be readily determinableby those of ordinary skill in the art.

The fabric should be exposed to the dye long enough for the fabric todye to the desired shade. The amount of time will depend on the exactcomposition of the fabric and will be readily determinable by thoseordinarily skilled in the art.

Following dyeing, typical aftertreatments may be used as are presentlyknown to those of ordinary skill in the art or are hereafter developed.These steps depend on the specific dyestuff or blend of dyestuffs usedand include, for example, after scouring.

Another aspect of the present invention is a heat and flame resistantchambray article that contains from about 20% to nearly 100% melaminefibers by weight. The melamine fibers are dyed with direct dyes (withoutusing salt), disperse dyes, non-metallized acid dyes or metallized aciddyes, or blends thereof. In addition to the melamine fiber, the fabriccontains cellulosic fibers selected from cotton fibers, rayon fibers,bast fibers, leaf fibers, and blends thereof. The cellulosic fibers aresubstantially not dyed (but may be stained) by the direct dye,non-metallized acid dye, or metallized acid dye used to dye the melaminefiber.

IV. DYED FABRICS (AND YARNS) FROM BLENDS OF MELAMINE FIBER AND ARAMIDFIBER (ARAMID DYED)

A further aspect of the present invention is a process for dyeing anarticle constructed from a blend of heat and flame resistant melaminefiber and aramid fiber wherein the aramid fiber is dyed but the melaminefiber is not substantially dyed. The article to be dyed is placed forabout 30 to about 120 minutes in a dyebath containing a basic dye orblend of dyes, sodium nitrate and a carrier. The dyebath is heated to atleast about 100° C. to about 190° C. (or more). This aspect of thepresent invention and fabrics made thereby are illustrated in Examples11A-11C.

The fabric (or yarn) is composed of melamine with other fibers selectedfrom m-aramid fibers and p-aramid fibers.

The fabric may be in any form: woven, nonwoven, knitted, etc. The blendlevel may be from about 20% to nearly 100% melamine fiber by weight.Preferably, the amount of melamine fiber in the blend will be no morethan about 60% by weight. Other fiber types could also be present.

The melamine fiber may be any melamine fiber, but is preferably amelamine-formaldehyde fiber that is essentially the condensation productof melamine and formaldehyde in a molar ratio of two moles offormaldehyde to one mole of melamine and containinghydroxyoxaalkylmelamines and, possibly, other additives in smallamounts. One suitable melamine fiber is Basofil® fiber available fromBASF Corporation, Mt. Olive, N.J.

The dye in the dye bath is one or more basic dyes. Sodium nitrate (orequivalent) and a carrier are also present. Suitable carriers includeacetophenone; methyl benzoate; benzaldehyde; benzyl alcohol; benzylalcohol/acetophenone mixtures; cyclohexanone;N-cyclohexyl-2-pyrrolidone; N-octyl pyrrolidone; N,N-diethyl(meta-toluamide); N,N-dimethylformamide; mixtures of N-butyl andN-isopropyl phthalimide; aryl ethers; and benzamides and dimethylamides.Examples of these include Polydyol NN; C-Prodye NM; Cadra NEX; Dymex;and Cindye NMX. Swelling agents such as N-methyl-2-pyrrolidone;N,N-dimethylacetamide; dimethylsulfoxide; and N,N-dimethylformamides mayalso be used.

Other materials may also be present in the dyebath according toconventional dyeing practice. These materials include, for example,leveling agents, anti-foaming agents, dispersing agents, lubricatingagents and chelating agents and combinations of these.

The temperature of the dyebath is in the range of about 100° C. to about190° C. (or more), and preferably at least about 120° C. The precisetemperature will depend on the dyestuff used and should be readilydeterminable by those of ordinary skill in the art.

The fabric will stay in the dyebath for a period of time that will alsodepend on the dyestuff and will be readily determinable by those ofordinary skill in the art. Typical times range from about 30 to about120 minutes.

After the dyeing step is complete and the fabric or yarn is dyed to thedesired shade, typical, optional, subsequent steps may be used. Forexample, after scouring may be used if desired for a particular result.

Surprisingly, it was discovered that the dyed fabric exhibits a uniquechambray appearance without any subsequent process steps (e.g.,stone-washing) that are often used to enhance a chambray effect.Surprisingly, the aramid fiber is dyed but the melamine fiber is not (itcould be stained) and the fabric exhibits a chambray appearance withoutfurther process steps.

Another related aspect of the present invention is a melamine/aramidfiber blend fabric. This fabric may be made according to the aboveprocess, and will exhibit a chambray appearance due to the dyeing of thearamid fiber but not the melamine fiber to any significant degree.

V. IMPROVED COMFORT MELAMINE FABRICS AND YARNS

Another feature of the present invention is a process for improving thecomfort of fabrics made from melamine fibers. As noted, these fabricsmay have a harsh hand. It was very surprising that this hand can besignificantly improved by certain dyeing or mock dyeing conditions. Thisaspect of the invention is illustrated in Examples 9A-D and 10. Theincreased comfort was especially surprising because it was thought thatdyeing makes the hand of dyed fabrics less desirable.

The process involves submerging melamine or melamine blend fabrics in anaqueous bath heated to more than about 70° C. for more than about 15minutes. The bath may be pure water or it may be a mock dyebath or adyebath. A mock dye bath may (but does not have to) contain leveling,dispersing, lubricating, chelating or pH adjustment agents. In otherwords, the mock dyebath may contain all of the chemicals present in adyebath, except the dyestuffs.

The dyebath may contain all of the usual chemicals present in a dyebath.It is not believed, however, that the specific amount and specific typeof additives in the dyebath is essential to the result.

The melamine fabric or yarn may be a blend of melamine with one or morem-aramid fibers, p-aramid fibers, glass fibers, carbon fibers, othermineral or ceramic fibers, steel fibers, polybenzimidazole fibers,polyimide fibers, polyamide-imide fibers, polytetraflouroethylenefibers, polyaryletherketone fibers, novoloid fibers, polyetheretherketone fibers, polyacrylate fibers; polyethersulfone fibers, poly(vinylchloride), poly(vinylidene chloride) fibers, polyvinyl alcohol fibers,nylon, polyester, liquid crystalline polyester fibers, natural andsynthetic cellulosic fibers such as cotton fibers, rayon fibers, bastfibers, leaf fibers, cellulose acetate fibers, FR versions of thesefibers, wool fibers (and other animal fibers), polyester fibers,modacrylic fibers, acrylic fibers, and various blends and combinationsof the above. The melamine may be present at from about 20% to nearly100% by weight of the fabric or yarn. In the case of fiber blendscontaining cotton fibers that probably will not later be treated with aflame retardant chemical, the melamine fiber is preferably present at alevel of at least about 60% by weight.

It is preferred that the bath be heated to from about 90° C. to about130° C. for at least about 60 minutes.

Moisture regain is one factor attributed to comfort in fabrics. Themoisture regain after such treatment will be greater than about 6.5%based on the weight of the melamine fiber in the fabric or yarn.Preferably, the regain after treatment will be at least about 8% toabout 9% based on the weight of the melamine fiber.

In addition to increasing the moisture regain of the melamine fabrics,the process of the present invention also increases the softness of thehand and the whiteness of uncolored melamine fabrics.

This invention will be described by reference to the following detailedexamples. The examples are set forth by way of illustration, and are notintended to limit the scope of the invention. All percentages are byweight unless otherwise indicated.

EXAMPLES 1A-1D p-Aramid/Melamine Fiber Blend Fabrics and Yarns-ChambrayAppearance

Fabric samples of 60% Basofil® melamine fiber (available from BASFCorporation, Mt. Olive, N.J.) and 40% p-aramid fiber (Twaron® availablefrom Akzo Nobel, Chicago, Ill.) constructed into an 8 oz/yd² plain weavefabric suitable for firefighter outer shell turn-out gear are scoured bythe following procedure and then used for the dyeings of Examples 1A-1D.

Scouring

The scouring step uses a 30:1 (bath:fabric) ratio. The bath contains:

demineralized water;

1.0 gram per liter Sandopan® LF nonionic polyalkylene oxide adduct(available from Clariant Corporation, Charlotte, N.C.); and

0.5 grams per liter soda ash.

The bath containing the fabric is heated to 70° C. and held at 70° C.for 20 minutes. Samples are then rinsed thoroughly in warm waterfollowed by cold water.

Example 1A: Dyeing with Direct Dye

The scoured fabric is dyed in a dyebath at a ratio of 20:1(dyebath:fabric) with a direct dye. The dyebath contains:

demineralized water;

1.0% Sandopan® LF; and

1.0% Intralite® Red 6BLL (C.I. Direct Red 79) (available from Crompton &Knowles Corporation, Charlotte, N.C.)

The bath pH is adjusted to 3.0 with acetic acid. The bath is heated at1.5° C. per minute to 135° C. and run at 135° C. for 60 minutes. Thebath is cooled and samples are rinsed thoroughly with warm and then coldwater. After rinsing, the sample is centrifugally extracted and hung ona line to dry.

Example 1B: Dyeing with Non-Metallized Acid Dye

The scoured fabric is dyed in a dyebath at a ratio of 20:1(dyebath:fabric) with a non-metallized acid dye. The dyebath contains:

demineralized water;

1.0% Chemcogen® AC anionic leveling agent (available from Rhone-Poulenc,Inc., Lawrenceville, Ga., under the trade name Supralev AC); and

1.0% Tectilon® Blue 4R (C.I. Acid Blue 277) (available from CibaCorporation, Greensboro, N.C.).

The bath pH is adjusted to 3.0 with acetic acid. The bath is heated at1.5° C. per minute to 135° C. and run at 135° C. for 60 minutes. Thebath is cooled and samples are rinsed thoroughly with warm and then coldwater. The rinsed sample is centrifugally extracted and hung on a lineto dry.

Example 1C: Dyeing with Metallized Acid Dye

The scoured fabric is dyed in a dyebath at a ratio of 20:1(dyebath:fabric) with a metallized acid dye. The dyebath contains:

demineralized water;

1.0% Uniperol® NB-SE leveling agent (available from BASF Corporation,Charlotte, N.C.); and

1.0% Irgalan® Blue 3GL 200% (C.I. Acid Blue 171) (available fromCrompton & Knowles Corporation, Charlotte, N.C.)

The bath pH is adjusted to 3.0 with acetic acid. The bath is heated at1.5° C. per minute to 135° C. and run at 135° C. for 60 minutes. Thebath is cooled and samples are rinsed thoroughly with warm and then coldwater. The sample is centrifugally extracted and hung on a line to dry.

Example 1D: Dyeing with Disperse Dye

The scoured fabric is dyed in a dyebath at a ratio of 20:1(dyebath:fabric) with a disperse dye. The dyebath contains:

demineralized water; and

1.0% Dipersol® Blue BG Grains (C.I. Disperse Blue 26)(available fromBASF Corporation, Charlotte N.C.).

The bath pH is adjusted to 4.5 with acetic acid. The bath is heated at1.5° C. per minute to 135° C. and run at 135° C. for 60 minutes. Thebath is cooled and samples are rinsed thoroughly with warm and then coldwater. The rinsed sample is centrifugally extracted and hung on a lineto dry.

The melamine fibers in the fabrics are dyed in Examples 1A-1D while thearamid fibers are not dyed to a significant degree. The fabrics exhibita pleasing chambray appearance and the hand is softer than before thedyeing procedure.

EXAMPLES 2A and 2B Producer-Colored p-Aramid/Melamine Fiber BlendFabrics and Yarns

Fabric samples of 40% of Basofil® melamine fiber and 60% black producercolored Kevlar® fiber (p-aramid fiber available from I.E. Du Pont deNemours, Wilmington, Del.) constructed in a fashion suitable forfirefighter outer shell turn-out gear are scoured by the following anddyed as follows.

Scouring

The scouring bath ratio is 15:1 (bath:fabric). The bath contains:

demineralized water;

0.50 % Kieralon® NB-OL anionic scouring agent (available from BASFCorporation, Charlotte, N.C.); and

0.50 % soda ash.

The bath is heated to 75° C. and held at 75° C. for 20 minutes. Thescoured fabrics are rinsed thoroughly in warm and then cold water.

Example 2A. Dyeing with Metallized Acid Dye

The scoured fabrics are dyed at a 15:1 (bath:fabric) ratio in a dyebathcontaining:

demineralized water;

1.0% Uniperol® NB-SE;

1.5 grams per liter of sodium acetate; and

0.6% Acidol® Black M-SRL dyestuff (C.I. Acid Black 194) (available fromBASF Corporation, Charlotte, N.C.).

The bath pH is adjusted to 3.0 with acetic acid. The bath is heated at1.5° C. per minute to 140° C. and run at 140° C. for 60 minutes. Thebath is cooled and samples are rinsed thoroughly with warm and then coldwater. The sample is centrifugally extracted and tumble dried.

Example 2B: Dyeing with Metallized Acid Dye

A scoured fabric is dyed as in Example 2A, except that the dyestuff is0.6% Acidol® Grey M-G (C.I. Acid Black 187) (available from BASFCorporation, Charlotte is N.C.).

The dyed fabrics of Examples 2A and 2B have a uniform black appearance.Also, the hand of the fabrics is softer after the dyeing process thanbefore.

EXAMPLES 3A and 3B m-Aramid/Melamine Fiber Blend Fabrics andYarns-Chambray Appearance

Fabrics of 40% of Basofil® melamine fiber and 60% Nomex® 450 fiber(m-aramid available from I.E. Du Pont de Nemours, Wilmington, Del.) isconstructed from as an 8 oz/yd² interlock knit fabric suitable for hoodgarments such as used by automobile race drivers or firefighters. Thesefabrics are scoured by the following procedure and dyed as described forExamples 3A and 3B.

Scouring

The fabrics are scoured in a 20:1 (bath:fabric) ratio in a bathcontaining:

demineralized water;

0.50 grams per liter Kieralon® NB-OL; and

0.50 grams per liter TSPP (tetrasodium pyrophosphate).

The bath is heated to 75° C. and held at 75° C. for 20 minutes. Thefabrics are rinsed thoroughly in warm and then cold water.

Example 3A: Dyeing with Metallized Acid Dye

The scoured fabrics are dyed at a ratio of 10:1 (bath:fabric) in a bathcontaining:

demineralized water;

2.0% Uniperol® NB-SE;

1.3 grams per liter sodium acetate; and

1.0% Lanaset Blue 2R dyestuff (available from Ciba Textile ProductsCorporation, Greensboro, N.C.).

The bath pH is adjusted to 3.0 with citric acid. The bath is heated at1.5° C. per minute to 130° C. and run at 130° C. for 60 minutes. Thebath is cooled and samples are rinsed thoroughly with warm and then coldwater. The sample is afterscoured by the following method.

Afterscouring

The afterscouring procedure is at a ratio of 10:1 (bath:fabric) in abath containing:

demineralized water; and

1.0 gram per liter Tanapon X-70 modified polyglycol ether (availablefrom Sybron Chemicals Inc., Welford, S.C.).

The bath pH is adjusted to 4.5 with acetic acid, heated to 85° C. andrun at 85° C. for 20 minutes. The bath is then cooled and samples arerinsed thoroughly with warm and then cold water. The sample iscentrifugal extracted and tumble dried.

Example 3B: Dyeing with Metallized Acid Dye

Another sample scoured and dyed by the procedures outlined in Example3A, except that the dyestuff is 1.0% Acidol Black M-SRL.

The melamine fibers are dyed in Examples 3A-3B. The fabrics exhibit apleasing chambray appearance and softer hand than before the dyeingprocess.

EXAMPLES 4A-4C m-Aramid/Melamine Fiber Blend Fabrics-Chambray Appearance

Fabrics of 50% of Basofil® melamine fiber and 50% Nomex® 462 (m-aramidavailable from I.E. Du Pont, Wilmington, Del.) are constructed as a 4.5oz/yd² plain weave fabric suitable for protective workwear apparelapplications. Samples of this fabric are scoured and dyed as outlinedbelow.

Scouring

The scouring is at a 10:1 (bath:fabric) ratio in a bath containing:

demineralized water;

0.50 grams per liter Kieralon® NB-OL; and

0.50 grams per liter soda ash.

The bath is heated to 75° C. and held at 75° C. for 20 minutes. Samplesare rinsed thoroughly in warm and then cold water.

Example 4A: Dyeing with Metallized Acid Dye

A fabric sample is dyed at a 15:1 (bath:fabric) ratio in a dyebathcontaining:

demineralized water;

3.0% Tanapal® BP leveling agent (available from Sybron Chemicals,Wellford, S.C.);

10.5% Lanaset® Grey G 50% dyestuff (no C. I. number) (available fromCiba Corporation, Greensboro, N.C.); and

1.68% Lanaset® Red G dyestuff (no C. I. number) (available from CibaCorporation, Greensboro, N.C.).

The bath pH is adjusted to 2.5 with citric acid. The bath is heated at1.5° C. per minute to 135° C. and run at 135° C. for 60 minutes. Thebath is cooled and samples are rinsed thoroughly with warm and coldwater. The samples are afterscoured by the following method:

Afterscouring

The afterscouring bath contains the fabric at a 10:1 (bath:fabric)ratio. The bath composition is:

demineralized water; and

1.0 gram per liter Tanapon® X-70.

The bath pH is adjusted to 4.5 with acetic acid. The bath is heated to75° C. and run at 75° C. for 20 minutes. The bath is cooled and samplesare rinsed thoroughly with warm and cold water. The samples arecentrifugally extracted and tumble dried.

Example 4B: Dyeing with Metallized Acid Dye

Another sample is scoured, dyed and afterscoured by the proceduresoutlined for Example 4A except that the dyestuff is 8.0% Acidol® BlackM-SRL.

Example 4C: Dyeing with Metallized Acid Dye

Another sample is scoured, dyed and afterscoured by the proceduresoutlined in Example 4A except that the dyestuff is 8.0% Lanaset® Black B(no C. I. number) (available from Ciba Corporation, Greensboro, N.C.)

The melamine fiber is dyed in Examples 4A-4C while the aramid fiber doesnot dye to any significant degree. The fabrics exhibit a pleasingchambray appearance and have a softer hand than before dyeing.

EXAMPLES 5A -5B

m-Aramid/Melamine Fiber Blend Yarns-Chambray Appearance

30s singles cotton count ring spun yarn of 50% Basofil® melamine fiberand 50% Nomex® 462 m-aramid fiber is circular knit into tubes andscoured and dyed as below.

Scouring

Scouring is at a 15:1 (bath:fabric) ratio in a bath containing:

demineralized water;

0.50 grams per liter Kieralon NB-OL; and

0.50 grams per liter soda ash.

The bath is heated to 75° C. and held at 75° C. for 20 minutes. Thescoured samples are rinsed thoroughly in warm and cold water.

Example 5A: Dyeing with Disperse Dye

demineralized water;

1.0% Palegal® NB-SF dyeing auxiliary for high temperature dyeing(available from BASF Corporation, Charlotte, N.C.);

0.25 grams per liter Versene® ethylenediaminetetraacetic acidtetrasodium salt chelating agent; and

4.0% Palanil® Blue R (C.I. Disperse Blue 56).

The bath pH is adjusted to 6.0 with acetic acid. The bath is heated at2.0° C. per minute to 140° C. and run at 140° C. for 60 minutes. Thebath is cooled and samples are rinsed thoroughly with warm and coldwater. The sample is then centrifugally extracted and tumble dried.

Example 5B. Dyeing with Metallized Acid Dye

Another sample is scoured by the procedures outlined for Example 5A anddyed in at a 15:1 (bath:fabric) ratio in a bath containing:

demineralized water;

3.0% Tanapal® BP leveling agent (commercially available from SybronChemicals Inc., Welford, S.C.); and

4.0% Lanaset® Black B dyestuff.

The bath pH is adjusted to 2.5 with citric acid. The bath is heated at2.0° C. per minute to 140° C. and run at 140° C. for 60 minutes. Thebath is cooled and samples are rinsed thoroughly with warm and coldwater. The sample is then centrifugally extracted and tumble dried.

The melamine fiber is dyed in Examples 5A and 5B while the aramid fiberdoes not dye to a significant degree. The fabrics exhibit a pleasingchambray effect and have a softer hand than before dyeing.

EXAMPLES 6A and 6B Wool/Melamine Fiber Blend Fabrics and Yarns

Fabric samples are prepared in a plain weave construction to give a 9oz./yd.² fabric containing (1) 60% Basofil® melamine fiber and 40% wool;or (2) 50% Basofil® melamine fiber and 50% wool; and (3) 40% Basofil® Pmelamine fiber and 60% wool. Fabric samples are dyed as described below:

Example 6A: Dyeing with Disperse Dye

The fabrics are each dyed in a bath at a 25:1 (bath:fabric) ratio in abath containing:

demineralized water;

1.5% Palegal® NB-SF;

0.25 grams per liter Versene®;

3.0% ammonium sulfate; and

4.0% Terasil® Brilliant Blue BGE (C.I. Disperse Blue 60) (available fromCiba Corporation, Greensboro, N.C.).

The bath pH is adjusted to 6.0 with acetic acid. The bath is heated at2.0° C. per minute to 110° C. and run at 110° C. for 45 minutes. Thebath is cooled and samples are rinsed thoroughly with warm and coldwater. Each fabric sample is then centrifugally extracted and linedried.

Example 6B: Dyeing With Disperse Dye

Each sample is dyed as in Example 6A except that the dyestuff is 1.5%Palanil® Red FFN (C.I. Disperse Red 279) (available from BASFCorporation, Charlotte, N.C.).

The melamine fibers are dyed in Examples 6A and 6B while the wool fibersdo not dye to a significant degree. The melamine/wool blend fabricsexhibit a pleasing chambray appearance and have a softer hand thanbefore dyeing.

EXAMPLES 7A-7F Cellulosic/Melamine Fiber Blend Yarns and Fabrics(Cellulose Dyed) (Chambray Appearance)

A 12 singles cotton count two-ply yarn sample is prepared consisting of60% of Basofil® melamine fiber and 40% cotton. The yarn is circular knitinto tubes or woven into a plain weave 10 oz/yd² and prepared and dyedas described below:

Example 7A: Cotton/Melamine Fiber Blend Dyed With Indigo Dye

Scouring

The circular knit yarn is scoured in a 20:1 (bath:fabric) ratio in abath containing:

demineralized water;

10.0% sodium hydroxide (50%); and

4 grams per liter Kieralon® NB-CD pretreatment chemical (available fromBASF Corporation, Charlotte, N.C.).

The bath is heated to 100° C. and held at 100° C. for 3 hours. Samplesare rinsed thoroughly in both hot and cold water.

Bleaching

Scoured knit yarn samples are bleached in a 10:1 (bath:fabric) ratio ina bath containing:

demineralized water;

2.0% Kieralon® NB-CD;

2.0% Prestogen TX-180 peroxide bleaching stabilizer (available from BASFCorporation, Charlotte, N.C.);

5.0% sodium hydroxide (50%); and

10.0% hydrogen peroxide (30%).

The bath is heated to 95° C. and held at 95° C. for 1 hour. The bath iscooled to approximately 50° C., dropped and a fresh bath is made asfollows. The bath ratio is 10:1 (bath:fabric).

demineralized water at 60° C.; and

1.0% Lufibrol® NB-7 extracting and dispersing agent for impurities incotton pretreatments (available from BASF Corporation, Charlotte, N.C.).

The second bath is heated to 65° C. and held at 65° C. for 10 minutes.The bath is cooled to approximately 50° C., dropped and a third freshbath is made and samples treated at a 10:1 (bath:fabric) ratio indemineralized water. The water bath is heated to 82° C. and held at 82°C. for 10 minutes. The bath is cooled to approximately 50° C., droppedand the samples rinsed with hot water for approximately 10 minutes. Thesamples are neutralized for 5 minutes in a fresh bath, at approximatelya 30:1 (bath:fabric) ratio. The pH is adjusted to 7.0 with acetic acid.The samples are then mercerized as follows:

Mercerizing

The bleached fabric is mercerized at a 20:1 (bath:fabric) ratio in abath containing:

demineralized water; and

40.0% sodium hydroxide (50%).

The samples are placed in the bath and stirred for 30 seconds. Thesamples are rinsed with deionized water twice at room temperature at a30:1 (bath:fabric) ratio. Samples are introduced to another deionizedwater bath at a 30:1 (bath:fabric) ratio. The pH off the new bath isadjusted to pH 6-7 with acetic acid. The samples are treated in the bathfor 5 minutes. Samples are then rinsed in hot and cold water,centrifugally extracted and line dried.

Simulated Continuous Dyeing

To 500cc of demineralized water at 35° C. is added;

0.5 grams per liter Albatex® OR (leveling and penetrating agent for vatdyes available from Ciba Corporation, Greensboro, N.C.);

15 grams per liter Sodium Hydroxide (50%);

6 grams per liter Indigo Pure (C.I. Vat Blue 1) (available from BASFCorporation, Charlotte, N.C.);

10 grams per liter sodium hydrosulfite; and

1 gram per liter Triton® X-100 (nonionic surfactant available from Rohmand Haas Company, Philadelphia, Pa.).

The fabric is dipped into the solution for 3-5 seconds and squeezedbetween rolls of a horizontal pad to achieve a wet pick up ofapproximately 100%. The sample is allowed to stand in air (oxidize) for60 seconds. The padding and oxidation are repeated 5 more times. Thesample is hand washed in warm water for 5 minutes in a bath containing 1gram per liter Tanapon® X-70. the samples are rinsed thoroughly in warmand cold water, centrifugally extracted and tumble dried.

Example 7B. Cotton/Melamine Fiber Blend Dyed With Vat Dye

Circular knit tubes are scoured, bleached and mercerized by theprocedures outlined in Example 7A. The dyeing procedure is as follows;

Exhaust Dyeing

The bath ratio is 20:1. The bath contains:

demineralized water at 55° C.;

0.5 grams per liter Albatex® OR;

15 grams per liter sodium hydroxide (50%)

7.5 grams per liter sodium hydrosulfite; and

2.5% Palanthrene® Brilliant Green FFB (C.I. Vat Green 1) (available fromBASF Corporation, Charlotte, N.C.).

The bath is stirred for 5 minutes before adding the fabric sample. Afteradding the fabric, the bath is heated to 60° C. and held at 60° C. for 1hour. The samples are rinsed thoroughly in warm water. The samples areaftertreated in a 30:1 (bath:fabric) ratio as follows;

demineralized water; and

1 gram per liter sodium perborate.

The aftertreatment bath is heated to 45° C. and run at 45° C. for 20minutes. The samples are then rinsed thoroughly with warm water andtreated 5 minutes in a bath of demineralized water to which 5 grams perliter acetic acid is added. The sample is rinsed thoroughly with coldwater, centrifugally extracted and tumble dried.

Example 7C: Cotton/Melamine Fiber Blends Dyed With Vat Dye

Circular knit tubes are scoured, bleached and mercerized by theprocedures outlined in Example 7A. The samples are dyed by theprocedures outlined in Example 7B, except that the dyestuff is 0.2%Palanthrene® Brown LBG (C.I. Vat Brown 84) (available from BASFCorporation, Charlotte, N.C.

Example 7D: Dyeing of Cotton/Melamine Fiber Blend With Direct Dye

Circular knit tubes or woven fabric from Example 6 are scoured, bleachedand mercerized by the procedures outlined in Example 7A except that thedyeing is done as follows;

Dyeing

The fabric is dyed at a 20:1 (bath:fabric) ratio. The bath contains:

demineralized water;

1.0% Intratex® DD leveling agent (available from Crompton & KnowlesColors, Inc., Charlotte, N.C.);

20% Glauber's salt (sodium sulfate);

0.4% Intralite® Brilliant Blue L (C.I. Direct Blue 98) (available fromCrompton & Knowles Colors, Inc., Charlotte, N.C.); and

4.0% Superlitefast® Yellow EFC (C.I. Direct Yellow 106) (available fromCrompton & Knowles Colors, Inc., Charlotte, N.C.).

The bath pH is adjusted to 6.0 with acetic acid. The bath is heated to95° C. and held at 95° C. for 1 hour. Samples are rinsed thoroughly inwarm and cold water, centrifugally extracted and tumble dried.

Example 7E: Cotton/Melamine Fiber Blend Dyed With Direct Dye

Circular knit tubes are scoured, bleached and mercerized by theprocedures outlined in Example 7A, dyed as in Example 7D, except thatthe following dyestuffs are used:

2.48% Intralite® Brilliant Blue L (C.I. Direct Blue 98) (available fromCrompton & Knowles Colors, Inc., Charlotte, N.C.);

0.27% Intralite® Scarlet BNLL (C.I. Direct Red 89) (available fromCrompton & Knowles Colors, Inc., Charlotte, N.C.);

1.13% Superlitefast® Yellow EFC (C.I. Direct Yellow 106) (available fromCrompton & Knowles Colors, Inc., Charlotte, N.C.).

Example 7F: Cotton/Melamine Fiber Blend Dyed With Naphthol Dye

Circular knit tubes are scoured, bleached and mercerized by theprocedures outlined in Example 7A and dyed as follows

Dyeing-Impregnation

Fabrics are treated at a 10:1 (bath:fabric) ratio in a bath containing:

demineralized water;

2.0 grams per liter Patogen Stabilizer NDA dyebath stabilizer (availablefrom Yorkshire Pat-Chem Inc., Greenville, S.C.);

8.0 grams per liter Naphtanilide® SG 50% Liq. (C.I. Azoic Coupler 13)(available from Yorkshire Pat-Chem Inc., Greenville, S.C.); and

7.0 grams per liter sodium hydroxide (50%)

The sample is tumbled in the bath for 40 minutes at room temperature,removed and centrifugally extracted.

Dyeing-Development

The fabrics are then dyed at a 10:1 (bath:fabric) ratio in a bathcontaining:,

demineralized water;

0.72 grams per liter Pat-Wet® Diazosperse dispersing agent (availablefrom Yorkshire Pat-Chem Inc., Greenville, S.C.); and

9.0 grams per liter Diazo Fast Red B (C.I. Diazo Component 5) (availablefrom Yorkshire Pat-Chem Inc., Greenville, S.C.).

The sample is tumbled in the bath for 40 minutes at room temperature,removed and rinsed warm and cold. The sample is then soaped by thefollowing procedure:

Soaping

The soaping is at a 10:1 (bath:fabric) ratio. The soaping bath contains:

demineralized water;

1.0 gram per liter soda ash; and

0.5 grams per liter Kieralon® TX-199 nonionic scouring agent (availablefrom BASF Corporation, Charlotte, N.C.).

The samples are heated to 60° C. and run at 6020 C. for 10 minutes. Thesamples are then placed in a fresh soaping bath with 2.0 grams per litersoda ash and 0.5 grams per liter Kieralon® TX-199. The samples areheated to 90° C. and run at 90° C. for 20 more minutes. Samples arefinally rinsed thoroughly in hot, warm and cold water, centrifugallyextracted and tumble dried. (Naphtanilide® SG 50% and Fast Red B arecommercially available from Yorkshire Pat-Chem Inc., Greenville, S.C.)

In Examples 7A-7F, the cotton fiber is dyed while the melamine fiber isnot substantially colored. The fabrics have a pleasing chambrayappearance.

EXAMPLE 8A-8D Cellulosic/Melamine Fiber Blend Yarns and Fabrics(Melamine Dyed) (Chambray Appearance)

Circular knit tubes as described in Example 7 are scoured, bleached andmercerized by the procedures outlined in Example 7. The tubes are thendyed by the following procedures;

Example 8A: Cotton/Melamine Fiber Blend Dyed With Disperse Dye

The sample is dyed at a 15:1 (bath:fabric) ratio in a bath containing:

demineralized water;

1.0% Palegal® NB-SF;

0.25% Versene; and

2.0% Terasil® Blue R.

The bath pH is adjusted to 5.0 with acetic acid. The bath is heated at2.0° C. per minute to 140° C. and run at 140° C. for 60 minutes. Thebath is cooled and samples are rinsed thoroughly with warm and coldwater. The sample is then centrifugally extracted and tumble dried.

Example 8B: Cotton/Melamine Blend Dyed With Disperse Dye

Circular knit tubes or woven fabric from Example 7 which are notscoured, bleached and mercerized are dyed by the procedure outlined inExample 8A after the following scour:

Scour

Samples are scoured at a 15:1 (bath:fabric) ratio in a bath containing:

demineralized water;

1.0% Kieralon® NB-OL; and

1.0% trisodium phosphate.

The bath is heated to 75° C. and run at 75° C. for 20 minutes. Followingthe scour, the samples are rinsed thoroughly with warm and cold water.

Example 8C: Cotton/Melamine Fiber Blends Dyed With Metallized Acid Dye

Circular knit tubes or woven fabric from Example 7 which are scoured,bleached and mercerized by the procedures outlined in Example 7A aredyed by the following procedure:

Dyeing

The samples are dyed at a 15:1 (bath:fabric) ratio in a bath containing:

demineralized water;

2.0% Uniperol NB-SE;

1.5 grams per liter sodium acetate; and

2.0% Acidol® Black M-SRL.

The bath pH is adjusted to 3.0 with citric acid. The bath is heated at2.0° C. per minute to 140° C. and run at 140° C. for 60 minutes. Thebath is cooled and samples are rinsed thoroughly with warm and coldwater. The sample is then centrifugally extracted and tumble dried.

Example 8D: Cotton/Melamine Fiber Blend Dyed With Metallized Acid Dye

Circular knit tubes or woven fabric from Example 7 which are notscoured, bleached and mercerized are dyed by the procedure outlined inExample 8C after the scouring procedure outlined in Example 8B. InExamples 8A-8D, the melamine fiber is dyed while the cotton fiber didnot dye to a significant degree. The samples have a pleasing chambrayappearance.

EXAMPLES 9A-9D Mock-Dyeing Melamine Yarns and Fabrics

Samples of an 18 oz/yd² plain weave fabric consisting of 100% by weightof Basofil® melamine fiber is scoured by the following procedure andmock-dyed in a bath containing dyeing auxiliaries but not dyestuff byvarious simulated dyeing conditions outlined below. Fabric hand andflexural rigidity are assessed and reported in TABLES 1 and 2 using alsoa scoured sample as Example 9.

Scouring (Example 9)

Samples are scoured at a 15:1 (bath:fabric) ratio in a bath containing:

demineralized water;

0.50 grams per liter Kieralon NB-OL; and

0.50 grams per liter soda ash;

The bath is heated to 70° C. and held at 70° C. for 20 minutes. Samplesare rinsed thoroughly in warm and cold water.

Example 9A: Simulated Melamine/Aramid Fiber Blend Dyeing

The fabric is mock-dyed at a 5:1 (bath:fabric) ratio in a bathcontaining;

demineralized water at 60° C.;

2.0% Uniperol® W dispersing and leveling agent (available from BASFCorporation, Charlotte, N.C.);

30 grams per liter Cindye® C-45 aryl ether dyeing assistant (availablefrom Stockhausen Inc., Greensboro, N.C.); and

15 grams per liter sodium nitrate.

The bath pH is adjusted to 2.5 with citric acid. The bath is heated at1.5° C. per minute to 135° C. and run at 135° C. for 20 minutes. Thebath is emptied at 70° C. and the sample is rinsed with hot and coldwater.

Example 9B: Simulated Melamine/Aramid Fiber Blend Dyeing

Scoured fabric samples are dyed by the procedures outlined in Example9A, except the time the dyebath is held at 135° C. is 60 minutes.

Example 9C: Simulated Melamine/Cellulosic Fiber Blend Dyeing

Scoured fabric samples are mock-dyed at a 15:1 (bath:fabric) ratio in abath containing:

demineralized water;

1.0% Intratex® DD; and

20% Glauber's Salt.

The pH is not adjusted. The bath is heated at approximately 3.0° C. perminute to 90° C. and run at 90° C. for 20 minutes. The bath is cooled,emptied and the sample is rinsed with hot and cold water.

Example 9D: Simulated Melamine/Cellulosic Fiber Blend Dyeing

Scoured fabric samples are dyed by the procedures outlined in Example9C, except the time the dyebath is held at 90° C. is 60 minutes.

The mock-dyed fabric samples of Examples 9A-9D and a scoured sample ofExample 9 are evaluated against an untreated fabric sample (100%melamine) as a control for characteristics which are believed tocontribute to increased comfort. These characteristics are fabric handby AATCC Evaluation Procedure 5; flexural rigidity by ASTM MethodD-1388-64; and moisture regain by AATCC Test Method 20A-1981. TABLE 1illustrates the results from AATCC Procedure 5-Fabric Hand: SubjectiveEvaluation of Fabrics. In this procedure, five observers rate the fabricsamples with respect to stiffness, pliability, softness, scratchinessand overall appeal compared to the untreated control. The samples arecoded so that the observers cannot identify the control. Observers sitin a room conditioned at 65+/-2% relative humidity and 70 +/-2 degreesFahrenheit to evaluate each treated sample against the untreatedcontrol. The samples are evaluated first on a flat surface, and then byhandling between the thumb and finger tips. Ratings are reported basedon the scale presented in TABLE 1. All observers rated all treatedsamples 9A-9D as less stiff, more pliable, softer and less scratchy thanthe untreated control.

                  TABLE 1                                                         ______________________________________                                        Assessment of Hand for Treated                                                Fabrics Averages from 5 Observers                                             Exam-                   More        Less                                      ple   Treatment                                                                              Less Stiff                                                                             Pliable                                                                             Softer                                                                              Scratchy                                                                             Overall                            ______________________________________                                        9     1        2.6      2.6   1.6   1.6    1.8                                9A    2        3.4      3.2   3.0   3.0    2.8                                9B    3        3.4      3.2   3.4   3.6    3.6                                9C    4        2.8      3.4   2.8   3.0    3.0                                9D    5        3.4      2.8   3.8   3.4    3.0                                ______________________________________                                         Treatments:                                                                   1 = Scoured                                                                   2 = Mock Dyed, pH 2.5 20 minutes, 35° C.                               3 = Mock Dyed, pH 2.5 60 minutes, 135° C.                              4 = Mock Dyed, 20 minutes, 90° C.                                      5 = Mock Dyed, 60 minutes, 90° C.                                      Ratings:                                                                      1 = No Difference                                                             2 = Slight Difference                                                         3 = Moderate Difference                                                       4 = Extreme Difference                                                   

The results indicate that fabrics 9A-9D show significant differences inindividual and overall hand of from the untreated control fabric.

TABLE 2 illustrates the results from ASTM Method D-1388-64 for flexuralrigidity. The results show that all mock-dyed fabrics 9A-9D haveflexural rigidity values that are about 3-9 times less than untreatedcontrol. Flexural rigidity is a measure of resistance to bending orstiffness. Lower flexural rigidity indicates lower resistance to bendingor improved "draping" properties.

                  TABLE 2                                                         ______________________________________                                        Fabric Stiffness Evaluation                                                                     Average                                                                       Overhang  Bending                                                                              Flexural Rigidity                          Example Treatment Length    Length (mg-cm)                                    ______________________________________                                        Control           6.4       3.2    2027.753                                   9       1         5.5       2.7    1255.232                                   9A      2         3.2       1.6    238.404                                    9B      3         3.2       1.6    245.281                                    9C      4         4.1       2.0    514.240                                    9D      5         4.1       2.1    537.319                                    ______________________________________                                         Treatments:                                                                   Control = untreated                                                           1 = Scoured                                                                   2 = Mock Dyed, pH 2.5, 20 minutes, 135° C.                             3 = Mock Dyed, pH 2.5, 60 minutes, 135° C.                             4 = Mock Dyed, 20 minutes, 90° C.                                      5 = Mock Dyed, 60 minutes, 90° C.                                 

TABLE 3 depicts results for moisture regain (as moisture content at 65%RH and 72° F) as measured by AATCC Test Method 20A-1981. The resultsindicate that mock-dyed samples have moisture regain about 2 to about 5percent higher than untreated samples and the scoured sample of Example9.

                  TABLE 3                                                         ______________________________________                                        Moisture Regain of Fabrics                                                    Example       Treatment                                                                              Moisture Regain                                        ______________________________________                                        Control                6.07                                                   9             1        7.5                                                    9A            2        10.12                                                  9B            3        9.53                                                   9C            4        8.67                                                   9D            5        8.38                                                   ______________________________________                                         Treatments:                                                                   Control = untreated                                                           1 = Scoured                                                                   2 = Mock Dyed, pH 2.5, 20 minutes, 135° C.                             3 = Mock Dyed, pH 2.5, 60 minutes, 135° C.                             4 = Mock Dyed, 20 minutes, 90° C.                                      5 = Mock Dyed, 60 minutes, 90° C.                                 

EXAMPLE 10 Mock-Dyed Melamine Fiber Fabric

A woven fabric of 100% Basofil® melamine fibers are mock-dyed accordingto the following process:

Scouring

The fabric is scoured in a bath to a weight ratio of 10:1 (bath:fabric).The bath contains:

demineralized water;

0.50 grams per liter Kieralon® NB-OL; and

0.50 grams per liter of TSPP.

The fabric is placed in the bath. The bath is heated to 75° C. and heldat 75° C. for 20 minutes. The fabric is removed from the bath and rinsedthoroughly in warm and then cold water.

Mock-Dyeing

Following scouring, the fabric is mock-dyed at a weight ratio of 10:1(bath:fabric). The bath contains:

demineralized water at 50° C.;

3.0% Tanapal® BP leveling agent;

15 grams per liter sodium nitrate; and

and 40 grams per liter Cindye® C-45.

The bath pH is adjusted to 2.5 with citric acid.

With the fabric in it, the bath is heated at 1.5° C. per minute to 135°C. and run at 135° C. for 60 minutes. The bath is emptied at 70° C. andthe sample is rinsed with hot and then cold water. The sample is thenafterscoured.

Afterscouring

The fabric is after scoured in a 10:1 (bath:fabric) ratio. The bathcontains:

demineralized water; and

1.0 gram per liter Tanapon® X-70.

The bath pH is adjusted to 4.5 with citric acid.

The bath containing the fabric is heated to 75° C. and run at 75° C. for20 minutes. The bath is cooled and samples are rinsed thoroughly withwarm and then cold water.

Physical Properties

Using a length of yarn taken from as-is fabric and a length of yarntaken from the mock-dyed fabric, the physical properties are measured.Denier is measured according to ASTM Method D-1907-89. Breaking load,tenacity, modulus at 3%, modulus at 5%, and breaking elongation, aremeasured by ASTM method D-2256-95A with the following results:

    ______________________________________                                                      Untreated Yarn                                                                         Mock-dyed yarn                                         ______________________________________                                        Denier          3996       5250                                               Cotton Count    1.3        1.0                                                Breaking load (gm)                                                                            2204.0     2035.0                                             Tenacity (gpd)  0.55       0.39                                               Modulus at 3% (gpd)                                                                           9.56       4.29                                               Modulus at 5% (gpd)                                                                           4.55       3.02                                               Breaking elongation (%)                                                                       9.3        11.1                                               ______________________________________                                    

EXAMPLE 11 Aramid/Melamine Fiber Blend Fabrics (Aramid Dyed) (ChambrayAppearance) Example 11A: Dyeing with Basic Dye

A 30s singles cotton count ring spun yarn sample of 50% by weight ofBasofil® melamine fiber and 50% Nomex® 462 m-aramid fiber is circularknit into tubes, scoured, dyed and afterscoured as outlined below.

Scouring

The knit tube is scoured in a bath at a weight ratio of 15:1(bath:fabric). The bath contains:

demineralized water;

0.50 grams per liter Kieralon NB-OL; and

0.50 grams per liter soda ash

The bath is heated to 75° C. and held at 75° C. for 20 minutes. Samplesare rinsed thoroughly in warm and cold water.

The scoured sample is placed into the dye vessel at a 15:1 (bath:fabric)ratio. The bath contains demineralized water at 60° C. Thirty (30) gramsper liter Cindye® C-45 is added to the bath. The bath is heated at 1.5°C. per minute to 75° C. and held for 15 minutes at 75° C. 2.0% Uniperol®W is added and the sample is held at 75° C. for 10 minutes. 2.0%Basacryl® Blue X-3GL (C.I. Basic Blue 41) (available from BASFCorporation, Charlotte, N.C.) is added and the sample is held at 75° C.for 10 minutes. 15 grams per liter Sodium Nitrate is added to the bathand the pH is adjusted to 2.5 with citric acid. The bath is heated at1.5° C. per minute to 135° C. and run at 135° C. for 60 minutes. Thebath is emptied at 70° C. and the sample is rinsed with hot and coldwater.

Afterscouring

The dyed knit tube is afterscoured at a 15:1 (bath:fabric) ratio in abath containing:

demineralized water; and

1.0 gram per liter Tanapon® X-70.

The bath pH is adjusted to 4.5 with acetic acid. The bath is heated to75° C. and run at 75° C. for 20 minutes. The bath is cooled and samplesare rinsed thoroughly with warm and cold water. The sample is thencentrifugally extracted and tumble dried.

Example 11B: Dyeing with Basic Dye

Another sample is scoured, dyed and afterscoured by the proceduresoutlined in Example 11A, except the dye is 2.0% Basacryl® Yellow X-2GL(C.I. Basic Yellow 65) (available from BASF Corporation, Charlotte,N.C.).

Example 11C: Dyeing with Basic Dye

Another sample is scoured, dyed and afterscoured by the proceduresoutlined in Example 11A, except the dye is 2.0% Basacryl® Red GL (C.I.Basic Red 29) (available from BASF Corporation, Charlotte, N.C.). InExamples 11A-11C, the aramid fiber is dyed while the melamine fiber isnot substantially colored. The fabrics have a pleasing chambrayappearance.

What is claimed is:
 1. A fabric comprising melamine fibers having amoisture regain of greater than 8% by weight of the melamine fiber inthe fabric as measured by AATCC Test Method 20A-1981.
 2. The fabric ofclaim 1 wherein said fabric is dyed.
 3. The fabric of claim 1 whereinsaid fabric comprises a blend of melamine fibers and other fibers. 4.The fabric of claim 3 wherein said blend contains from 20% to nearly100% by weight of melamine fibers.
 5. The fabric of claim 1 wherein saidmelamine fibers are melamine-formaldehyde fibers comprising thecondensation product of melamine and formaldehyde in a molar ratio oftwo moles of formaldehyde to one mole melamine; one or morehydroxyoxaalkylmelamines.
 6. The fabric of claim 3 wherein said otherfibers are selected from the group consisting of: m-aramid fibers,p-aramid fibers, glass fibers, carbon fibers, ceramic fibers, steelfibers, polybenzimidazole fibers, polytetraflouroethylene fibers,polyaryletherketone fibers, novoloid fibers, polyethersulfone fibers,polyimide fibers, polyamideimide fibers, polyetherether ketone,polyacrylate fibers, poly(vinyl chloride), poly(vinyl alcohol) fibers,poly(vinylidene chloride) fibers, nylon fibers, liquid crystallinepolyester fibers, cotton fibers, rayon fibers, bast fibers, leaf fibers,cellulose acetate fibers, wool, cashmere, rabbit, silk mohair, acrylicfibers, modacrylic fibers, flame retardant versions of these fibers, andvarious blends and combinations thereof.